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Chemical Structure| 947144-53-8 Chemical Structure| 947144-53-8

Structure of 947144-53-8

Chemical Structure| 947144-53-8

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Product Details of [ 947144-53-8 ]

CAS No. :947144-53-8
Formula : C6H2ClF3N2O3
M.W : 242.54
SMILES Code : O=C1C([N+]([O-])=O)=C(Cl)C=C(C(F)(F)F)N1
MDL No. :MFCD22574137

Safety of [ 947144-53-8 ]

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H301-H311-H331
Precautionary Statements:P261-P264-P270-P271-P280-P302+P352-P304+P340-P310-P330-P361-P403+P233-P405-P501
Class:6.1
UN#:2811
Packing Group:

Application In Synthesis of [ 947144-53-8 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 947144-53-8 ]

[ 947144-53-8 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 947144-26-5 ]
  • [ 947144-53-8 ]
YieldReaction ConditionsOperation in experiment
<strong>[947144-26-5]3-Nitro-6-trifluoromethyl-pyridine-2,4-diol</strong> (5.8 gm, 26 mmol) was heated in phenylphosphonic dichloride (3OmL) at 1000C for 19 hours. Cooled and poured on to ice (60 gm), extracted with ethyl acetate (3 x 50 mL). The combined organic extracts were washed with aqueous sodium hydrogen carbonate solution (10%w/v) until the washings remained basic (pH ~8). The deep yellow organic layer was then washed with saturated brine, dried over sodium sulphate, filtered and evaporated to give a yellow gum. Trituration of the gum with dichloromethane gave a yellow solid which was filtered off and dried (4.65gm). The solid was dissolved in water (25mL) and acidified with 2N hydrochloric acid (7.5mL) to give a thick white precipitate which was filtered off and washed with water. The precipitate was dissolved in ethyl acetate, dried over sodium sulphate, filtered and evaporated to give 4-chloro-3-nitro-6-trifluoromethyl- pyridin-2-as a white solid (3.75gm).
PREPARATION 34; 4-Chloro-3-nitro-6-trifluoromethyl-pyridin-2-ol; <strong>[947144-26-5]3-Nitro-6-trifluoromethyl-pyridine-2,4-diol</strong> (5.8 gm, 26 mmol) was heated in phenylphosphonic dichloride (30 mL) at 100 C. for 19 hours. The resulting mixure was then cooled and poured on to ice (60 gm), and then extracted with ethyl acetate (3×50 mL). The combined organic extracts were washed with aqueous sodium hydrogen carbonate solution (10% w/v) until the washings remained basic (pH 8). The deep yellow organic layer was then washed with saturated brine, dried over sodium sulphate, filtered and evaporated to give a yellow gum. Trituration of the gum with dichloromethane gave a yellow solid which was filtered off and dried (4.65 gm). The solid was dissolved in water (25 mL) and acidified with 2N hydrochloric acid (7.5 mL) to give a thick white precipitate which was filtered off and washed with water. The precipitate was dissolved in ethyl acetate, dried over sodium sulphate, filtered and evaporated to give the title compound as a white solid (3.75 gm).1H NMR (DMSOd6) 7.78 (s, 1H). 13C NMR (DMSOd6) 157.2 (s) 145.2 (q) 138.1 (s) 136.98 (s) 120.6 (q) 113.86 (s). LRMS (ES-) m/z 241/243 [MH]-
 

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